IP 470/05

Determination of aluminium, silicon, vanadium, nickel, iron,

calcium, zinc and sodium in residual fuel oil by ashing, fusion
and atomic absorption spectrometry

This standard does not purport to address all of the safety problems associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability
of regulatory limitations prior to use.

FOREWORD encouraged to investigate the possibility of applying

The technique is essentially the same as that
described in IP 377, with more elements being
analyzed, and new precision values. The precision
values for aluminium and silicon are taken from
IP 377.
1 Scope
This standard specifies a procedure for the
determination of aluminium, silicon, vanadium,
nickel, iron, calcium, zinc and sodium in residual fuel
oils, at levels detailed in the table below, by atomic
absorption spectrometry.
the most recent editions of the normative
documents indicated. For undated references, the
latest edition of the normative document referenced
applies.
ISO 648, Laboratory glassware — One-mark
pipettes.
ISO 835-2, Laboratory glassware — Graduated
pipettes- Part 2: Pipettes for which no waiting time
is specified.
ISO 1042, Laboratory glassware — One-mark
volumetric flasks.

IP 475, Petroleum liquids — Manual sampling.

Element Range mg/kg
(/ ISO 3170)
Aluminium 5 to 150
Silicon 10 to 250 IP 476, Petroleum liquids — Automatic pipeline
sampling. (/ ISO 3171)
Vanadium 1 to 400
Nickel 1 to 100 ISO 3696, Water for analytical laboratory use —
Iron 2 to 60
Specification and test methods.

Sodium 1 to 100 ISO 3819, Laboratory glassware — Beakers.

Calcium 3 to 100
ISO 4788, Laboratory glassware — Graduated
Zinc 1 to 70
measuring cylinders.

Aluminium and silicon are normally found in
association with each other in residual fuels, and
may be specified, separately or in combination, as
an estimate of catalyst fines content.
2 Normative references
The following normative documents contain
provisions which, through reference in this text,
constitute provisions of this standard. For dated
references, subsequent amendments to, or revisions
of, any of these publications do not apply. However,
parties to agreements based on this standard are
IP 367, Petroleum products — Determination and
application of precision data in relation to methods
of test. (/ ISO 4259)
3 Principle
A weighed test portion, together with an ashing
agent, is ignited and burnt, and the residual carbon
removed by heating in a muffle furnace. The residue
is fused with a dilithium tetraborate/lithium fluoride
flux and the fused mixture digested in a solution of
tartaric acid and hydrochloric acid. For vanadium a

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 Al, Si, V, Ni, Fe, Ca, Zn, Na IN FUEL OIL - AAS, IP 470

Lanthanum based interference suppressant is added. 4.9 Tartaric acid

After dilution with water, the solution is aspirated
into the flame of an atomic absorption spectrometer
(AAS) and the absorption of the resonance radiation
of the elements under analysis is measured, and
compared to a calibration curve constructed from
standard calibration solutions.
NOTE 1 - The ashing agent is required only for samples
with sulphur content less than 0,3 % m/m.
4.9.1 Tartaric acid/hydrochloric acid solution.
Dissolve 5 g of tartaric acid in approximately
500 ml of water acidified with 40 ml of hydrochloric
acid (4.7) and dilute to 1 000 ml with water.
4.10 Nitric acid
Concentrated, 70 % (m/m) HNO3.

4 Reagents and materials 4.10.1 Nitric acid solution (1 + 1). Mix equal
volumes of nitric acid (4.10) and water.
4.1 General
4.11 Lanthanum Chloride solution
All reagents shall be of analytical reagent grade or
of higher purity and water shall be of at least grade 4.11.1 Lanthanum/hydrochloric acid solution
3 purity as specified in ISO 3696.
Dissolve 60 ± 1 g La2O3in approx. 600 ml water
4.2 Potassium hydrogensulfate (KHSO4) and 200 ml hydrochloric acid solution (1 + 4)
(4.7.3) in a 1 000 ml volumetric flask. Make up to
Fused solid. the mark with water.

4.3 Ashing agent Or

Sulfur, 99,9 % (m/m) minimum purity. 4.11.2 Lanthanum chloride solution

4.4 Propan-2-ol Dissolve 135 ± 1 g of LaCl3. 7H2O in 600 ml water

in a 1 000 ml volumetric flask. Make up to the mark
4.5 Toluene with water.

4.6 Toluene/propan-2-ol mixture (1 + 1) NOTE 2 - It may be necessary to add hydrochloric acid

solution (1+4) (4.7.3) to the lanthanum chloride solution
to assist in solubility.
Mix equal volumes of toluene and propan-2-ol.

4.7 Hydrochloric acid 4.12 Standard solutions

Concentrated, 36 % (m/m) HCl. 4.12.1 Aluminium standard solution. Use either a

commercially available aluminium standard solution
4.7.1 Hydrochloric acid solution (1 + 1). Mix of 1 000 mg/l aluminium content, or prepare in the
equal volumes of hydrochloric acid (4.7) and water. manner described in 4.12.1.1.

4.7.2 Hydrochloric acid solution (1 + 2). Mix one
volume of hydrochloric acid (4.7) with two volumes
of water.
4.7.3 Hydrochloric acid solution (1+4). Mix one
volume of hydrochloric acid (4.7) with four volumes
of water.
4.8 Flux
Mixture of 90 % (m/m) dilithium tetraborate
(Li2B4O7) and 10 % (m/m) lithium fluoride (LiF).
4.12.1.1 Dissolve 1 000 g ± 0,001 g of aluminium
metal wire, of minimum purity 99,9 % Al, in 50 ml
hydrochloric acid (4.7) with gentle heating in a
400 ml beaker (5.13). Cool, transfer to a 1 000 ml
volumetric flask (5.9), and dilute to the mark with
water.
4.12.2 Silicon standard solution. Use either a
commercially available silicon standard solution of
1 000 mg/l silicon content, or prepare in the manner
described in 4.12.2.1.

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 Al, Si, V, Ni, Fe, Ca, Zn, Na IN FUEL OIL - AAS, IP 470
4.12.2.1 Fuse 2,140 g ± 0,001 g of silicon
dioxide, of minimum purity 99,99 % SiO2, with
8 g of sodium hydroxide in a zirconium crucible
fitted with a close-fitting lid (5.4) at dull red heat
until a clear melt is obtained. Cool and dissolve the
solidified melt in 100 ml of hydrochloric acid
solution (4.7.2) in a 400 ml beaker (5.13). Cool,
transfer to a 1 000 ml volumetric flask (5.9), make
up to the mark with water, followed by immediate
transfer to a plastic bottle (5.15) for longer-term
storage.
4.12.3 Vanadium standard solution. Use either a
commercially available vanadium standard solution
of 1 000 mg/l vanadium content, or prepare in the
manner described in 4.12.3.1.
4.12.3.1 Dissolve 1 000 g ± 0,001 g of vanadium
metal, of minimum purity 99,9 % V, in 40 ml of
nitric acid (4.10) with gentle heating in a 400 ml
beaker (5.13). Cool, transfer to a 1 000 ml
volumetric flask (5.9) and make up to the mark with
water.
4.12.4 Nickel standard solution. Use either a
commercially available nickel standard solution of
1 000 mg/l nickel content, or prepare in the manner
described in 4.12.4.1.
4.12.4.1 Dissolve 1,000 g ± 0,001 g of nickel
metal of minimum purity 99,9 % Ni, in 40 ml of
nitric acid solution (4.10.1) with gentle heating in a
400 ml beaker (5.13). Cool, transfer to a 1 000 ml
volumetric flask (5.9) and make up to the mark with
water.
4.12.5 Iron standard solution. Use either a
commercially available iron standard solution of
1 000 mg/l iron content, or prepare in the manner
described in 4.12.5.1.
4.12.5.1 Dissolve 1,000 g ± 0,001 g of iron metal
of minimum purity 99,9 % Fe, in 40 ml of
hydrochloric acid solution (4.7.1) with gentle
warming in a 400 ml beaker (5.13). Cool, transfer to
a 1 000 ml volumetric flask (5.9) and make up to
the mark with water.
4.12.6 Sodium standard solution. Use either a
commercially available sodium standard solution of
1 000 mg/l sodium content, or prepare in the
manner described in 4.12.6.1.
4.12.6.1 Dissolve 2,542 g ± 0,001 g of sodium
chloride (NaCl) in water in a 400 ml beaker (5.13).
Transfer to a 1 000 ml volumetric flask (5.9), make
up to the mark with water, and mix.
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4.12.7 Calcium standard solution. Use a
commercially available calcium standard solution of
1 000 mg/l calcium content.
4.12.7.1 Dissolve 2,498 g ± 0,001 g of calcium
carbonate (CaCO3) in water in a 400 ml beaker
(5.13) with 100 ml water and add dropwise 10 ml
of hydrochloric acid solution (4.7.1). Transfer to a
1 000 ml volumetric flask (5.9), make up to the
mark with water, and mix.
4.12.8 Zinc standard solution. Use a commercially
available zinc standard solution of 1 000 mg/l zinc
content.
4.12.8.1 Dissolve 1 000 g ± 0,001 g of zinc metal
in minimum volume of hydrochloric acid solution
(1 + 1)(4.7.1) in a 400 ml beaker (5.13). Transfer
to a 1 000 ml volumetric flask (5.9), make up to the
mark with water, and mix.
5 Apparatus
5.1 General
The apparatus requirements are detailed in 5.2 to
5.16. All glassware and the zirconium crucible shall
be sodium-free and carefully cleaned with hot
hydrochloric acid solution (4.7.1) and rinsed
thoroughly with water to eliminate contamination.
5.2 Atomic absorption spectrometer
Use an instrument with a modulated hollow cathode
lamp or other source of modulated resonance
radiation of sodium/aluminium/silicon/ vanadium/
nickel/iron/calcium/zinc. It shall be fitted with an
air/acetylene burner, a dinitrogen oxide (nitrous
oxide)/acetylene burner, and a light detector with a
suitable measuring and readout system. The scale
shall be linear in absorbance, or of light intensity.
5.3 Platinum basin
Of 100 ml capacity with a minimum diameter of
70 mm. Clean the basin with fused potassium
hydrogensulfate (4.2).
NOTE 3 - The following cleaning technique is
recommended: place approximately 5 g of potassium
hydrogensulfate (4.2) in the basin, heat in a muffle
furnace at 550 °C ± 25 °C or over a Bunsen burner for
5 min. Allow to cool, wash out with water and dry.
An alternative cleaning technique is to use hot
hydrochloric acid (4.7.1.) however the precision of this
method is based on the potassium hydrogen sulphate
technique only.
 Al, Si, V, Ni, Fe, Ca, Zn, Na IN FUEL OIL - AAS, IP 470

5.4 Zirconium crucible requirements of ISO 4788.

Of a capacity of 30 ml to 50 ml, and fitted with a 5.13 Beaker

close-fitting zirconium lid.
400 ml capacity, squat form, complying with the
5.5 Mixer requirements of ISO 3819.

Non-aerating, high-speed type. 5.14 Filter paper

5.6 Oven 'Ashless' grade, 0,01 % (m/m) ash content

maximum.
Electric, capable of being maintained at a
temperature between 50 °C and 60 °C. 5.15 Plastic bottles

5.7 Muffle furnace
Electric, capable of being maintained at
temperatures of 525 °C ± 25 °C and 925 °C ±
25 °C, and preferable having apertures at front and
rear to allow passage of a slow, natural draught of
air. Ensure that the refractory walls are in good
condition, with no loose particles.
5.8 Hot plate
Electric, with or without a magnetic stirring
capability.
5.9 Volumetric flasks
100 ml, 25 ml and 1 000 ml capacity, complying
with the requirements of ISO 1042, class A.
5.10 Pipettes
1 ml, 2 ml, 5 ml, 10 ml, 20 ml and 25 ml capacity,
complying with the requirements of ISO 658, class
A.
NOTE 4 - Auto-dispensing pipettes may be used as an
alternative provided that they meet the requirements
detailed above.
5.11 Pipettes
1 ml and 2 ml capacity, graduated in 0,1 ml
subdivisions, complying with the requirements of
ISO 835-2.
NOTE 5 - Auto-dispensing pipettes may be used as an
alternative provided that they meet the requirements
detailed above.
5.12 Measuring cylinders
10 ml, 25 ml, 50 ml and 100 ml capacity, with
subdivided graduations, complying with the
100 ml and 1 000 ml capacity, suitable for long-
term storage of dilute acid solutions.
5.16 Analytical balance
Capable of weighing to the nearest 0,2 mg.
6 Samples and sampling
6.1 Unless otherwise specified, laboratory
samples shall be obtained by the procedures
described in IP 475 or IP 476.
6.2 Thoroughly mix samples in their containers
immediately prior to withdrawal of the test portions.
Place the sample container in the oven (5.6) and
maintain the sample at 50 °C to 60 °C until all the
sample is fluid and of uniform viscosity. Insert the
shaft of the mixer (5.5) into the sample container so
that the head of the shaft is immersed to
approximately 5 mm from the bottom of the
container. Mix the sample for approximately 5 min.
6.3 Efficient mixing of the sample is essential to
the accuracy and precision of this test method.
Hand shaking alone will invalidate results.
7 Procedure
7.1 Test portion mass
Select a mass of test portion, between 20 g and
50 g, to yield approximately 1,3 mg of aluminium.
NOTE 6 - The mass of test portion selected based on the
aluminium content, will suffice for the silicon
determination as both elements are usually found in
residual fuels associated with each other. Where the
levels of other elements are low, it may be necessary to
take the maximum mass (50 g) of test portion, and dilute
the test solutions as required for the aluminium and
silicon determinations.

470.4
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 Al, Si, V, Ni, Fe, Ca, Zn, Na IN FUEL OIL - AAS, IP 470
7.2 Test solution preparation
7.2.1 Immediately after homogenization, transfer
the test portion from the container to the weighed
platinum basin (5.3). Re-weigh the basin and
contents to the nearest 0,1 g to obtain the test
portion mass.
7.2.2 If the sulphur content of the sample is below
0,3 % m/m add 0,3 g of ashing agent (4.3) to the
basin, distributing it as evenly as possible over the
surface of the basin contents.
Prepare a blank test portion containing only the
ashing agent, and use it for the complete procedure
in this clause.
7.2.3 Warm the basin and contents gently with a
Bunsen flame until the test portion ignites. Maintain
the contents of the basin at a temperature such that
most of the combustible material is removed and
only carbon and ash remain.
NOTE 7 - If the sample contains considerable amounts of
moisture, foaming and frothing may cause loss of test
portion.
If foaming and frothing occur, discard the test
portion and add 1 ml to 2 ml of propan-2-ol (4.4)
before heating. If foaming and frothing are not
sufficiently reduced, add 10 ml of toluene/propan-2-
ol mixture (4.6) to a further test portion and mix
thoroughly. Place several strips of filter paper (5.14)
in the mixture before warming gently.
NOTE 8 - When the paper begins to burn, the greater part
of the water will have been removed.
7.2.4 Place the basin and its contents in the
muffle furnace (5.7), preheated to a temperature of
525 °C ± 25 °C. Ensure that the basin contents
are not contaminated with refractory from the
furnace walls, as this will contribute to erroneous
silicon results. Maintain the muffle furnace at this
temperature until all the carbon has been removed
and only ash remains.
NOTE 9 - This may take overnight.
7.2.5 Cool the basin to room temperature, add
0,4 g of flux (4.8), and mix it with the ash. Place
the basin and contents in the muffle furnace
preheated to a temperature of 925 °C ± 25 °C for
5 min. Remove the basin and ensure contact of the
flux with the ash. Replace the basin in the muffle
furnace and maintain the temperature at 925 °C ±
25 °C for a further 10 min.
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7.2.6 Remove the basin and cool the fusion melt
to room temperature. Add 50 ml tartaric
acid/hydrochloric acid solution (4.9.1) to the basin
and place on the hot plate (5.8). Maintain at a
moderate temperature without boiling.
NOTE 10 - Excessive evaporation of the solution could
lead to precipitation of an insoluble form of silica.
NOTE 11 - Prolonged heating may be required to dissolve
the solidified melt completely and obtain a solution.
Agitation, or the use of magnetic stirring may be
employed to speed dissolution of the solidified melt.
7.2.7 Allow the solution to cool and then transfer
it to a 100 ml volumetric flask (5.9) with water,
washing the basin several times to ensure that the
transfer is quantitative. Make up to the mark with
water, and transfer immediately to a 100 ml plastic
bottle (5.15).
7.2.8 For vanadium determination only, transfer
5,0 ml of the lanthanum solution (4.11.1 or 4.11.2)
into a 25 ml volumetric flask and fill to the mark
with the test solution (7.2.7)
NOTE 12 - Transfer to a plastic bottle is thought to be
desirable as the dilute acid solution will contain
tetrafluoroboric acid (HBF4) from solution of flux.
However, storage tests have shown that there is no
attack of glassware in the short term (up to one week),
and that the solution does not contain free fluoride 'ion'
above the 5 mg/l level.
7.3 Preparation of blank solution
7.3.1 Prepare a blank solution containing only
0,4 g flux (4.8) and 50 ml of the tartaric
acid/hydrochloric acid solution (4.9.1), diluted to
100 ml, and transfer immediately to a 100 ml
plastic bottle (5.15).
7.3.2 Vanadium blank solution. Prepare a zero-
concentration solution containing 0,3 g flux, 50 ml
of the tartaric acid/hydrochloric acid solution (4.9.1)
and 20 ml of the lanthanum solution (4.11.1 or
4.11.2) diluted to 100 ml and transfer immediately
to 100 ml plastic bottle.
7.4 Preparation of calibration solutions
7.4.1 Aluminium and silicon. Prepare a 250 mg/l
aluminium or silicon working solution by diluting
25 ml of the 1 000 mg/l standard solution (4.11.1
or 4.11.2) to 100 ml with water. To each of four
clean 100 ml volumetric flasks (5.9), add 0,4 g flux
(4.8) and 50 ml of the tartaric acid/hydrochloric acid
solution (4.9.1). To successive flasks add
 Al, Si, V, Ni, Fe, Ca, Zn, Na IN FUEL OIL - AAS, IP 470

2 ml, 4 ml, 10 ml and 20 ml of the 250 mg/l
aluminium or silicon working solution and dilute to
100 ml with water.
NOTE 13 - The calibration solutions contain 5 mg/l,
10 mg/l, 25 mg/l and 50 mg/l of aluminium or silicon
respectively.
7.4.2 Nickel, iron, sodium, calcium and zinc.
Prepare a 100 mg/l nickel, iron, sodium, calcium or
zinc working solution by diluting 10 ml of the
1 000 mg/l standard solution (4.12.4, 4.12.5,
4.12.6, 4.12.7 or 4.12.8) to 100 ml with water. To
each of four clean 100 ml volumetric flasks (5.9),
add 0,4 g flux (4.8) and 50 ml of the tartaric
acid/hydrochloric acid solution (4.9.1). To
successive flasks add 5 ml, 10 ml, 15 ml and 20 ml
of the 100 mg/l calcium, zinc, nickel, iron or sodium
working solution and dilute to 100 ml with water.
NOTE 14 - The calibration solutions contain 5 mg/l,
10 mg/l, 15 mg/l and 20 mg/l of calcium, zinc, nickel, iron
or sodium respectively.
7.4.3 Vanadium. Prepare a 100 mg/l vanadium
working solution by diluting 10 ml of the 1 000 mg/l
standard solution (4.10.3) to 100 ml with water. To
each of four clean 100 ml volumetric flasks (5.9),
add 0,3 g flux (4.8), 50 ml of the tartaric
acid/hydrochloric acid solution (4.9.1) and 20 ml of
the lanthanum solution (4/11/1 or 4.11.2). To
successive flasks add 5 ml, 10 ml, 15 ml and
20 ml of the 100 mg/l vanadium working solution
and dilute to 100 ml with water.
NOTE 15 - The calibration solutions contain 5 mg/l,
10 mg/l, 15 mg/l and 20 mg/l of vanadium.
7.4.4 Storage. Transfer all standards immediately
after preparation to 100 ml plastic bottles (5.15).
7.5 Setting up the spectrometer
7.5.1 General. Consult and follow the
manufacturer’s instructions for the operation of the
atomic absorption spectrometer (5.2).
NOTE 16 - Design differences between spectrometers
make it impracticable to specify the required
manipulations.
WARNING - Correct operating procedures are
required for safety as well as for reliability of
results. An explosion can result from flame blow-
back unless the correct burner head and operating
sequence are used.
7.5.2 Settings. Fit the hollow cathode lamp for the
element of interest and set the lamp current to that
recommended by the manufacturer. Set the
monochrometer to the specified wavelength (see
Table 1) and adjust the wavelength control to get
maximum output.

Table 1 - Instrument settings

Element Wavelength Fuel Oxidant

nm
Aluminium 309,3 Acetylene Dinitrogen oxide
(nitrous oxide)
Silicon 251,6 Acetylene Dinitrogen oxide
(nitrous oxide)
Vanadium 318,5 Acetylene Dinitrogen oxide
(nitrous oxide)
Nickel 232,0 Acetylene Air

Iron 248,3 Acetylene Air

Sodium 589,0 Acetylene Air

Calcium 422,7 Acetylene Dinitrogen oxide
(nitrous oxide)
Zinc 213,9 Acetylene Air

470.6
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 Al, Si, V, Ni, Fe, Ca, Zn, Na IN FUEL OIL - AAS, IP 470
Using the burner fuel and oxidant as specified in
Table 1, aspirate a calibration solution (7.4.1 or
7.4.2 e.g. 25 mg/l) into the flame. Make
adjustments to burner height, burner alignment, fuel
gas flow rate and impact bead to give maximum
absorbance (or minimum transmittance). Adjust the
gain control to set the maximum within the
recommended working region of the spectrometer
(see manufacturer’s operating instructions).
7.5.3 Calibration curve. Prepare a calibration curve
prior to analysis of each group of samples and after
any change in instrumental conditions, as variations
occur in the instrument behaviour. The mode of
calibration depends on the type of readout facility
on the instrument.
NOTE 17 - Readings may vary over short times from such
causes as buildup of deposits on the burner slot or in the
nebulizer. The visual appearance of the flame is a useful
check to detect changes of condition.
7.5.4 Analysis of the test solution. Analyze one of
the calibration standards after every fifth test
sample. If the result indicates that the calibration
has changed by greater than 5% drift (see note 14),
recalibrate the instrument.
If it is found that a test solution gives a metal
content above the highest content of any calibration
solution, dilute it in the same matrix, i.e. blank
solution (7.3), to bring it within the range of
calibration solutions.
To ensure that analysis is carried out within linear
calibration, the metal content in the final analysis
solution shall not exceed 10 mg/l for vanadium and
sodium.
7.5.4.1 Spectrometers with meter readout. Aspirate
the calibration solution, blank solution and test
solution sequentially into the flame and record the
meter reading. Aspirate the blank solution between
each test solution.
If the spectrometer output is linear in absorbance,
plot a calibration graph of net absorbance
(calibration solution absorbance minus blank solution
absorbance) against element content in mg/l. From
this calibration graph, estimate the element content
of each sample solution after similarly computing its
net absorbance.
If the spectrometer output is proportional to
transmission (i.e. light intensity), calculate the net
absorbance, A, using the following equation:
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(d0)
A = lg Õ
(d1)
where
d0 is the meter reading given by the
blank solution;
d1 is the meter reading given by the
calibration solution or test solution.
7.5.4.2 Spectrometers with digital readout and
built-in (non-microprocessor-controlled) curvature
correction and scale expansion facilities. Follow the
manufacturer’s operating instructions aspirating the
appropriate calibration solution, to set the digital
readout to read directly in the required units,
carrying out a curvature correction programme if
necessary.
Aspirate the test solution and read the element
content of each test solution and solution blank
directly from the readout given by the digital display
from the spectrometer.
7.5.4.3 Spectrometers with digital readout
microprocessor-controlled calibration facilities.
Follow the manufacturer’s operating instructions,
aspirating the appropriate calibration solution and
using the recommended calibration programme to
obtain a direct readout in element content; the
element content of each test and blank solution can
thus be directly obtained after aspiration of the test
solution.
8 Calculation
Calculate E, the content of the element of interest
as Al, Si, V, Ni, Fe, Ca, Zn or Na respectively in
milligrams per kilogram from the following equation:
100cd
E = ÕÕÕ
m
where
c is the element content of interest in
mg/l as read from the calibration
graph or direct readout;
d is the dilution factor, calculated
from the volumes and aliquots taken
to produce the test solution;
m is the mass of the test portion, in
grams.
NOTE 18 - Dilution factor, d, for vanadium is 1,25 (25 ml/20
ml) unless no further dilution procedures are carried out.
 Al, Si, V, Ni, Fe, Ca, Zn, Na IN FUEL OIL - AAS, IP 470

9 Expression of results identical test material would, in the normal and

Report the element content of each element of
interest to the nearest 1 mg/kg.
10 Precision
10.1 General
The precision given in 10.2 and 10.3 for elements
other than aluminium and silicon was determined by
statistical examination by IP 367 of interlaboratory
test results on a matrix of residual fuels that was
also used for the precision evaluation of the same
range of elements by inductively coupled plasma
emission spectrometry, and given in IP 501. The
values for aluminium and silicon are taken from IP
377.
10.2 Repeatability, r
The difference between two successive test results
obtained by the same operator with the same
apparatus under constant operating conditions on
correct operation of the test method, exceed the
value given in Table 2 only in one case in twenty.
10.3 Reproducibility, R
The difference between two single and independent
results obtained by different operators working in
different laboratories on nominally identical test
material would, in the normal and correct operation
of the test method, exceed the values given in Table
2 only in one case in twenty.
NOTE 19 - Reproducibility for calcium. During the
interlaboratory data collecting exercise it was found that
the level of bias between laboratories for this element
resulted in there being only 26 degrees of freedom. This
is fewer than the 30 required by IP 367 and users should
take note of this when testing for the calcium content of
fuel oils.
As a guide to users precision values for various
amounts of the elements have been calculated from
Table 2 and these are given in Table 3.

Table 2 - Precision values

Element Repeatability Reproducibility

mg/kg mg/kg

Aluminium 0,296 8 x0,67 0,789 0 x0,67

Silicon 0,353 9 x0,67 1,388 x0,67
Vanadium 0,742 x0,5 3,26 x0,5
Nickel 0,788 x0,55 2,333 x0,55
Iron 0,861 x0,6 1,887 x0,6
Sodium 0,597 x0,6 1,303 x0,6
Calcium 0,093 (x+14) 0,125 (x+28)
Zinc 0,265 x0,75 0,580 x0,75

where x is the average of the results being compared, in mg/kg.

Table 3 - Examples of actual precision

Zn Ca Na Fe Ni V
mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg
mg/kg r R r R r R r R r R r R
1 0,26 0,58 0,60 1,30 0,79 2,33 0,75 3,26
10 1,49 3,26 2,23 4,75 2,38 5,19 3,43 7,51 2,80 8,28 2,37 10,31
50 4,97 10,91 5,95 9,75 6,25 13,62 9,00 19,73 6,77 20,06 5,29 23,04
100 10,60 16,00 9,47 20,64 9,92 29,37 7,48 32,59
200 10,58 46,09
300 12,96 56,44
400 14,96 65,18

470.8
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 Al, Si, V, Ni, Fe, Ca, Zn, Na IN FUEL OIL - AAS, IP 470

11 Test report

The test report shall contain at least the following

information:

a) a reference to this standard;

b) all details necessary for complete

identification of the product tested;

c) the result of the test (see clause 9);

d) any deviations, by agreement or otherwise,

from the procedures specified;

e) the date of the test.

470.9
This document is issued with a single user licence to the EI registered subscriber: kemapro@aol.com
IMPORTANT: This document is subject to a licence agreement issued by the Energy Institute, London, UK. It may only be used in accordance with
the licence terms and conditions. It must not be forwarded to, or stored, or accessed by, any unauthorised user. Enquiries: e:pubs@energyinst.org t:
+44 (0)207 467 7100